CN102234353A - Preparation method of D113 dilute acid acrylic cation-exchange resin - Google Patents
Preparation method of D113 dilute acid acrylic cation-exchange resin Download PDFInfo
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- CN102234353A CN102234353A CN2011100996305A CN201110099630A CN102234353A CN 102234353 A CN102234353 A CN 102234353A CN 2011100996305 A CN2011100996305 A CN 2011100996305A CN 201110099630 A CN201110099630 A CN 201110099630A CN 102234353 A CN102234353 A CN 102234353A
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Abstract
The invention discloses a preparation method of D113 dilute acid acrylic cation-exchange resin. In the method, acrylonitrile, divinylbenzene, toluene, formyl and the like serve as main raw materials; and the D113 dilute acid acrylic cation-exchange resin is prepared by process steps of polymerization and hydrolysis.
Description
Technical field
The present invention relates to the preparation technology of ion exchange resin, specifically, is a kind of preparation method of D 113 weak acid acrylic acid type cation exchange resins.
Background technology
Exchange resin is mainly used in the extraction of tungsten, molybdenum, vanadium etc. in pure water, high purity water preparation, wastewater treatment, biochemical product extraction, rare metal extraction, the hydrometallurgy, has characteristics such as physical strength is good, thermotolerance height.
Summary of the invention
The object of the invention is to provide a kind of preparation method of D113 weak acid acrylic acid type cation exchange resin.
The present invention seeks to realize by following technique means:
A kind of preparation method of D113 weak acid acrylic acid type cation exchange resin comprises the steps:
One, polymerization:
1, charging capacity: vinyl cyanide 358kg, divinylbenzene 42kg, toluene 120kg, formyl 4kg.
2, operation steps:
(1) by a certain percentage water is prepared, stirred 20 minutes;
(2) stop to stir, the monomer that mixes is added start stir, look the granularity situation and mix up rotating speed;
(3) slowly be warming up to 60 ℃, observe spheroid granularity and typing situation;
(4) heat release of when typing is stronger, notes cooling, maintains the temperature at 70 ℃ after the heat release, is incubated 2 hours;
(5) with being warming up to 82 ℃ half an hour, be incubated 3 hours;
(6) be warming up to 96 ℃ with 1 hour, be incubated 5 hours;
(7) use the hot water wash nodule number all over till limpid to water;
(8) drain water, oven dry, sub-sieve is standby.
Two, hydrolysis:
1, charging capacity: Archon 400kg, sulfuric acid 1600L (content 50%～60%).
2, operation steps:
(1) in reactor, adds the sulfuric acid that specified quantity has prepared, add Archon again, start stirring;
(2) temperature rise rate with 2 ℃～3 ℃/min is warming up to 130 ℃, is incubated 12 hours, and it is qualified greater than 44% to survey moisture;
(3) be cooled to 45 ℃, be washed to neutrality;
(4) filter is done, no free-water packing.
Embodiment
Below in conjunction with embodiment the present invention is further described, but be not in order to limit the present invention.
Embodiment 1:
Be prepared as follows D113 weak acid acrylic acid type cation exchange resin:
One, polymerization:
1, charging capacity: vinyl cyanide 358kg, divinylbenzene 42kg, toluene 120kg, formyl 4kg.
2, operation steps:
(1) by a certain percentage water is prepared, stirred 20 minutes;
(2) stop to stir, the monomer that mixes is added start stir, look the granularity situation and mix up rotating speed;
(3) slowly be warming up to 60 ℃, observe spheroid granularity and typing situation;
(4) heat release of when typing is stronger, notes cooling, maintains the temperature at 70 ℃ after the heat release, is incubated 2 hours;
(5) with being warming up to 82 ℃ half an hour, be incubated 3 hours;
(6) be warming up to 96 ℃ with 1 hour, be incubated 5 hours;
(7) use the hot water wash nodule number all over till limpid to water;
(8) drain water, oven dry, sub-sieve is standby.
Two, hydrolysis:
1, charging capacity: Archon 400kg, sulfuric acid 1600L (content 50%～60%).
2, operation steps:
(1) in reactor, adds the sulfuric acid that specified quantity has prepared, add Archon again, start stirring;
(2) temperature rise rate with 2 ℃～3 ℃/min is warming up to 130 ℃, is incubated 12 hours, and it is qualified greater than 44% to survey moisture;
(3) be cooled to 45 ℃, be washed to neutrality;
(4) filter is done, no free-water packing.
Claims (1)
1. the preparation method of D 113 weak acid acrylic acid type cation exchange resins is characterized in that, comprises the steps:
(1) polymerization:
(1) charging capacity: vinyl cyanide 358kg, divinylbenzene 42kg, toluene 120kg, formyl 4kg;
(2) operation steps:
1. by a certain percentage water is prepared, stirred 20 minutes;
2. stop to stir, the monomer that mixes is added start stir, look the granularity situation and mix up rotating speed;
3. slowly be warming up to 60 ℃, observe spheroid granularity and typing situation;
Heat release is stronger when 4. finalizing the design, and notes cooling, maintains the temperature at 70 ℃ after the heat release, is incubated 2 hours;
5. with being warming up to 82 ℃ half an hour, be incubated 3 hours;
6. be warming up to 96 ℃ with 1 hour, be incubated 5 hours;
7. use the hot water wash nodule number all over till limpid to water;
8. drain water, oven dry, sub-sieve is standby;
(2) hydrolysis:
(1) charging capacity: Archon 400kg, sulfuric acid 1600L (content 50%～60%);
(2) operation steps:
1. in reactor, add the sulfuric acid that specified quantity has prepared, add Archon again, start stirring;
2. the temperature rise rate with 2 ℃～3 ℃/min is warming up to 130 ℃, is incubated 12 hours, and it is qualified greater than 44% to survey moisture;
3. be cooled to 45 ℃, be washed to neutrality;
4. filter is done, no free-water packing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100996305A CN102234353A (en) | 2011-04-20 | 2011-04-20 | Preparation method of D113 dilute acid acrylic cation-exchange resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100996305A CN102234353A (en) | 2011-04-20 | 2011-04-20 | Preparation method of D113 dilute acid acrylic cation-exchange resin |
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| CN102234353A true CN102234353A (en) | 2011-11-09 |
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| CN2011100996305A Pending CN102234353A (en) | 2011-04-20 | 2011-04-20 | Preparation method of D113 dilute acid acrylic cation-exchange resin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659968A (en) * | 2012-05-17 | 2012-09-12 | 定南县松源化工有限责任公司 | Hydrolysis technology for acrylic weak-acid cation exchange resin |
| CN102816341A (en) * | 2012-08-30 | 2012-12-12 | 中国石油天然气股份有限公司 | Synthetic method for weak-acid adsorption resin suitable for heavy oil wastewater |
| CN103008026A (en) * | 2012-11-27 | 2013-04-03 | 安徽皖东化工有限公司 | Preparation method of strong-alkaline acrylic anion exchange resin |
| CN105837742A (en) * | 2016-05-17 | 2016-08-10 | 张国华 | Preparation method of polyamide adsorption resin |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4500652A (en) * | 1981-08-21 | 1985-02-19 | Mitsubishi Chemical Industries, Limited | Process for producing cation exchange resins without swelling during sulphonation process |
| EP0406648A1 (en) * | 1989-07-06 | 1991-01-09 | Bayer Ag | Process for the preparation of weakly acid cation-exchanger resins |
| CN1082945A (en) * | 1993-05-27 | 1994-03-02 | 南开大学高分子化学研究所 | Weak-acid cation-exchange resin |
| CN1320647A (en) * | 2001-01-05 | 2001-11-07 | 南京大学 | Process for preparing macroreticular weakly acidic cationic exchange resin of acrylic series |
| CN101781382A (en) * | 2009-12-31 | 2010-07-21 | 安徽皖东化工有限公司 | Preparation method of 201*7 strong-basicity styrene series anion exchange resin |
-
2011
- 2011-04-20 CN CN2011100996305A patent/CN102234353A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4500652A (en) * | 1981-08-21 | 1985-02-19 | Mitsubishi Chemical Industries, Limited | Process for producing cation exchange resins without swelling during sulphonation process |
| EP0406648A1 (en) * | 1989-07-06 | 1991-01-09 | Bayer Ag | Process for the preparation of weakly acid cation-exchanger resins |
| CN1082945A (en) * | 1993-05-27 | 1994-03-02 | 南开大学高分子化学研究所 | Weak-acid cation-exchange resin |
| CN1320647A (en) * | 2001-01-05 | 2001-11-07 | 南京大学 | Process for preparing macroreticular weakly acidic cationic exchange resin of acrylic series |
| CN101781382A (en) * | 2009-12-31 | 2010-07-21 | 安徽皖东化工有限公司 | Preparation method of 201*7 strong-basicity styrene series anion exchange resin |
Non-Patent Citations (4)
| Title |
|---|
| 《黑龙江商学院学报自然科学版》 20000331 马旭等 "丙烯腈共聚物水解制备羧酸型阳离子交换树脂的研究" 第16卷, 第1期 * |
| 《黑龙江大学自然科学学报》 19891231 马俊山等 "丙烯腈共聚物水解制备羧酸型阳离子交换树脂的研究" , 第2期 * |
| 马俊山等: ""丙烯腈共聚物水解制备羧酸型阳离子交换树脂的研究"", 《黑龙江大学自然科学学报》, no. 2, 31 December 1989 (1989-12-31) * |
| 马旭等: ""丙烯腈共聚物水解制备羧酸型阳离子交换树脂的研究"", 《黑龙江商学院学报自然科学版》, vol. 16, no. 1, 31 March 2000 (2000-03-31) * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659968A (en) * | 2012-05-17 | 2012-09-12 | 定南县松源化工有限责任公司 | Hydrolysis technology for acrylic weak-acid cation exchange resin |
| CN102816341A (en) * | 2012-08-30 | 2012-12-12 | 中国石油天然气股份有限公司 | Synthetic method for weak-acid adsorption resin suitable for heavy oil wastewater |
| CN103008026A (en) * | 2012-11-27 | 2013-04-03 | 安徽皖东化工有限公司 | Preparation method of strong-alkaline acrylic anion exchange resin |
| CN103008026B (en) * | 2012-11-27 | 2015-12-23 | 安徽皖东化工有限公司 | The preparation method of strong basicity acrylic acid type anion exchange resin |
| CN105837742A (en) * | 2016-05-17 | 2016-08-10 | 张国华 | Preparation method of polyamide adsorption resin |
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Application publication date: 20111109 |